Organic silicon flame-retardant carbon-forming agent and preparation method thereof

A char-forming agent and organosilicon technology, which is applied in the field of silicon-containing cage-like flame-retardant char-forming agent compounds and their preparation, can solve the problems of no cost-effective char-forming agent or flame-retardant char-forming agent, etc. The effect of good capacitance and simple preparation method

Active Publication Date: 2012-10-24
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there is no good cost-effective carbon forming agent or flame retardant char forming agent

Method used

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  • Organic silicon flame-retardant carbon-forming agent and preparation method thereof
  • Organic silicon flame-retardant carbon-forming agent and preparation method thereof
  • Organic silicon flame-retardant carbon-forming agent and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Example 1 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device, add 0.1mol (13.42g) trimethylolpropane and 40ml acetonitrile, start stirring, and at 25 0.1 mol (14.95 g) of methyltrichlorosilane was added dropwise within about 30 minutes at ℃, and after the drop was completed, the temperature was raised to 65 ℃ and refluxed for 1 hour. Then the temperature was raised to 80°C for reflux reaction for 18 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered, and dried to obtain 1-methyl-4-ethyl-1-sila-2,6,7-trioxabicyclo [2,2,2]-Octane White solid. Its yield is 92%, and its decomposition temperature is 370±10°C.

Embodiment 2

[0047] Example 2 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device, add 0.1mol (13.42g) of trimethylolpropane and 40ml of dioxane, and start stirring , at 25°C, add 0.1mol (14.95g) methyltrichlorosilane dropwise within about 30min, and then raise the temperature to 65°C and reflux for 1h after the dropwise completion. Then the temperature was raised to 102°C for reflux reaction for 15 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered, and dried to obtain 1-methyl-4-ethyl-1-sila-2,6,7-trioxabicyclo [2,2,2]-Octane White solid. Its yield is 93%, and its decomposition temperature is 370±10°C.

Embodiment 3

[0048] Example 3 In a 100ml four-necked flask equipped with a stirrer, a thermometer, a dropping funnel, a reflux condenser and a hydrogen chloride absorption device, add 0.1mol (13.42g) trimethylolpropane and 40ml toluene, start stirring, and at 25 0.1 mol (14.95 g) of methyltrichlorosilane was added dropwise within about 30 minutes at ℃, and after the drop was completed, the temperature was raised to 65 ℃ and refluxed for 1 hour. Then the temperature was raised to 112°C for reflux reaction for 15 hours. After the hydrogen chloride was released, it was crystallized by cooling, filtered, and dried to obtain 1-methyl-4-ethyl-1-sila-2,6,7-trioxabicyclo [2,2,2]-Octane White solid. Its yield is 93%, and its decomposition temperature is 370±10°C.

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Abstract

The invention relates to an organic silicon flame-retardant carbon-forming agent 1-methyl-4-ethyl-1-silicon hetero-2,6,7-trioxygen hetero double-cycle[2,2,2]-octane compound and a preparation method thereof. The structure of the compound is shown as the following formula in the specification. The preparation method comprises the following step of reacting methyl trichlorosilane or methyltrimethoxy silane with trimethylolpropane in an organic solvent to prepare the 1-methyl-4-ethyl-1-silicon hetero-2,6,7-trioxygen hetero double-cycle[2,2,2]-octane. The organic silicon flame-retardant carbon-forming agent belongs to a halogen-free and non-toxic flame-retardant carbon-forming agent, has high flame-retardant performance and high carbon-forming property, can effectively prevent materials from melting and dropping off, has stable physical and chemical properties, high compatibility with a macromolecular material, low cost and a simple process, and is easy in industrialized production.

Description

technical field [0001] The invention relates to a silicon-containing cage flame-retardant char-forming agent compound and a preparation method thereof, in particular to 1-methyl-4-ethyl-1-sila-2,6,7-trioxabicyclo[2, 2,2]-octane and a preparation method thereof, the compound can be used as a flame-retardant char-forming agent for materials such as polyolefins, polyesters, polyurethanes, coatings and the like. Background technique [0002] With the advancement of science and technology and the improvement of people's living standards, the application of synthetic polymer materials has become more and more extensive, and it has also led to the rapid development of flame retardant materials. Flame retardants have become the second largest additives in plastic additives. With the advancement of technology, the requirements for flame retardants are getting higher and higher. High-efficiency, halogen-free, non-toxic, smoke-free, and anti-dripping flame retardants have become a hot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C08K5/549
Inventor 王彦林游基飞王乐然
Owner SUZHOU UNIV OF SCI & TECH
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